CN106323921B - A kind of transfer of interface photoelectron and the active assay method of material light catalysis and four-dimensional microscopic image analysis instrument - Google Patents

A kind of transfer of interface photoelectron and the active assay method of material light catalysis and four-dimensional microscopic image analysis instrument Download PDF

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CN106323921B
CN106323921B CN201610887230.3A CN201610887230A CN106323921B CN 106323921 B CN106323921 B CN 106323921B CN 201610887230 A CN201610887230 A CN 201610887230A CN 106323921 B CN106323921 B CN 106323921B
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electron
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acceptor molecule
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slit
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CN106323921A (en
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钟鸿英
张娟
姜若葳
张文洋
唐雪妹
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Huazhong Normal University
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    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited

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Abstract

The invention belongs to analytical chemistry fields, and in particular to a kind of transfer of interface photoelectron and the active assay method of material light catalysis and four-dimensional microscopic image analysis instrument.The four-dimension microscopic image analysis instrument includes sample target, laser, slit, extraction pole, six grades of bars, level four bars, time-of-flight mass analyzer, detector, the device for providing voltages to sample target, slit, extraction pole and six grades of bars.The present invention generates the tunnel-effect of light induced electron and the capture principle of electron acceptor molecule using semi-conducting material under laser irradiation, the mass-to-charge ratio and ion signal of interfacial migration light induced electron or electron acceptor molecule capture interfacial migration light induced electron initiation photochemical reaction products therefrom are captured by measuring electron acceptor molecule, and the micro-imaging in photocatalytic activity site is obtained by image reconstruction, on the one hand it may determine that semi-conducting material photocatalytic activity site, on the other hand it may determine that photochemically reactive difficulty or ease and gained photochemical reaction product occur for electron acceptor molecule.

Description

A kind of transfer of interface photoelectron and the active assay method of material light catalysis and four-dimensional aobvious Micro- imaging analysis instrument
Technical field
The invention belongs to analytical chemistry fields, and in particular to a kind of interface photoelectron transfer and material light catalysis are active Assay method and four-dimensional microscopic image analysis instrument.
Background technology
The transfer of biphase interface photoelectron is the key link in light-catalyzed reaction, the real-time monitoring of heterogeneous electron transfer process Understanding solar energy conversion, environmental contaminants light degradation etc. are played with the measurement of light-catalyzed reaction intermediates and reaction product Important function.Interface photoelectron transfer at present and the active assay method of material light catalysis include three categories:(1) whole mean value Method, such as Surface enhanced Raman spectroscopy method and fluorescent spectrometry.This method cannot reflect the single photocatalytic activity site of material Difference, cannot identify unknown light-catalyzed reaction product or intermediate product;(2) single molecular fluorescence spectroscopic methodology, this method utilize Target product caused by light-catalyzed reaction (such as superoxide anion) and fluorescence caused by probe molecule, although can be to list A photocatalytic activity site carries out high-resolution fluorescence imaging, but cannot identify unknown light-catalyzed reaction product or intermediate product; (3) scanning electron microanalyzer, this method requires sample to be in high vacuum state, therefore cannot reflect real reaction condition Under the transfer of interface photoelectron and photocatalytic activity and its change with time.
Invention content
The present invention is directed to the deficiencies in the prior art, and it is an object of the present invention to provide a kind of transfer of interface photoelectron and material light The assay method of catalytic activity and four-dimensional microscopic image analysis instrument.
For achieving the above object, the technical solution adopted in the present invention is:
One kind is for measuring interface photoelectron transfer and the active four-dimensional microscopic image analysis instrument of material light catalysis, feature Be, including be sequentially arranged sample target, laser, slit, extraction pole, six grades of bars, level four bars, time-of-flight mass analyzer And detector, further include the device that voltage is provided to sample target, slit, extraction pole and six grades of bars, the laser is used for sample Product target emission pulse laser, there are electrostatic fields, the time-of-flight mass analyzer to be used between the sample target~six grade bar Ion mass-to-charge ratio is measured, the detector is for detecting ion signal intensity and then obtaining photocatalytic activity by image reconstruction The micro-imaging in site.
In said program, the sample target and laser are in sample bin, and sample bin is atmospheric pressure;It is described narrow Seam, extraction pole, six grades of bars, level four bars, time-of-flight mass analyzer and detector are in vacuum system.
In said program, electrostatic electron lens is set between sample target and slit, the focusing for realizing ion and biography Defeated, the electrostatic electron lens is in sample bin, and sample bin is atmospheric pressure.
In said program, the four-dimension microscopic image analysis instrument further includes control system, for controlling pulse laser and quiet The synchronization or delay of electric field.
A kind of transfer of interface photoelectron and the active assay method of material light catalysis, include the following steps:
(1) laser parameter is set:According to the property of semi-conducting material and energy gap size, correspondingly optical maser wavelength is selected, is made Material energy gap is less than laser photon energy;
(2) electrostatic field parameters are set:Electrostatic field, sample target are set according to the property of semi-conducting material and electron acceptor molecule The light induced electron that voltage difference between slit can be such that semiconductor material surface generates obtains enough energy and tunnelling occurs, and electric The ion generated after sub- acceptor molecule capture photoelectron is focused in the electrostatic field between-six grades of bars of slit and transmission;
(3) it prepares semi-conducting material suspension to be measured or the semi-conducting material of different crystal faces is pasted on to conductive metal The semi-conducting material exposed with a variety of crystal faces is prepared on aluminium strip or copper strips;
(4) cleaning sample target draws semi-conducting material hanging drop to be measured in sample target surface, then naturally dry exists Electron acceptor molecule solution, naturally dry is added dropwise in semiconductor material surface;Or impregnate covering tool with electron acceptor molecule solution There are many semi-conducting materials of crystal face exposure, after natural drying, will adsorb being exposed with a variety of crystal faces for electron acceptor molecule Semi-conducting material be fixed on sample target, crystal face to be measured is upward;
(5) sample target is put into sample bin, opens laser to sample target emission pulse laser, adjusts electrostatic field, make half Conductor material generate interfacial migration light induced electron, electron acceptor molecule capture interfacial migration light induced electron obtain cation and/or Anion;
(6) under anionic textiles pattern, gained anion is transported in electrostatic field to high potential direction in step (5) It is dynamic, it passes through slit, extracted plate, six grades of bars and level four bars to focus, ion matter lotus is finally measured by time-of-flight mass analyzer Than detecting ion signal intensity by detector and obtaining the micro-imaging in photocatalytic activity site by image reconstruction;When in It is all that cation moves in electrostatic field to low potential direction in step (5) under positive ion detection pattern, pass through slit, warp It extracts plate, six grades of bars and level four bars to focus, ion mass-to-charge ratio is finally measured by time-of-flight mass analyzer, is detected by detector Ion signal intensity and the micro-imaging that photocatalytic activity site is obtained by image reconstruction.
In said program, electron acceptor molecule capture interfacial migration light induced electron include mating type electron capture, from Solution type electron capture and electron detachment.
In said program, the mating type electron capture is to form anion after electron acceptor molecule captures light induced electron; The dissociation type electron capture is that initiation specific chemical key fracture acquisition fragment is negative after electron acceptor molecule captures light induced electron Ion, the electron detachment occur electron detachment after interacting with electron acceptor molecule for the light induced electron of high-speed motion and obtain Obtain cation.
In said program, the semi-conducting material is selected from SiO2、BiOCl、Ce2O3、ZnO、BN、AlN、TiO2And Ga2O3In One kind.
In said program, the electron acceptor molecule is selected from Nucin, 4,4 '-DDT or aliphatic acid.
In said program, the electrostatic field size is adjustable, can it is synchronous with pulse laser or delay, to carry out light induced electron With the dynamics research of neutral molecule interaction.
In said program, the tunable wave length of the laser, spot size is tunable, and pulse frequency and width are adjustable Humorous, laser incident angle is tunable, can be with electrostatic field synchronization or delay to scan more crystal faces.
In said program, the solvent of the semi-conducting material suspension is isopropanol, a concentration of 10mg/mL.
In said program, the solvent of the electron acceptor molecule solution is acetone, a concentration of 5mg/mL.
In the present invention, for different samples, the composition of sample target cleaning solution may be different, common sample target cleaning solution group At including 50% (v/v) acetone and 50% (v/v) n-hexane.
The bearing calibration of anionic textiles pattern of the present invention is as described below:Semi-conducting material to be measured is prepared as suspending Liquid (10mg/mL) is dripped in sample target naturally dry;By Fatty acid standards drop in material surface, after natural drying, by sample target It is put into sample bin, sample bin is set as authentic dummy status, sets laser, electrostatic field and time-of-flight mass analyzer parameter, Laser scans sample target is opened, the matter lotus of anion caused by the photoelectron of electron acceptor molecule capture interfacial migration is measured Than and signal strength, corrected with this.The bearing calibration phase of the bearing calibration of positive ion detection pattern and anionic textiles pattern Together.The Fatty acid standards liquid is formulated as:Including nine kinds of free fatty C6:0, C8:0, C10:0, C12:0, C14:0, C16:0, C18:0, C20:0 and C22:0, these aliphatic acid are dissolved in n-hexane so that a concentration of 5mg/ of these aliphatic acid mL。
Beneficial effects of the present invention:
(1) present invention using semi-conducting material generated under laser irradiation light induced electron macroscopical tunnel-effect and electronics by The capture principle of body molecule captures interfacial migration light induced electron (anion) or electron acceptor point by measuring electron acceptor molecule The mass-to-charge ratio and ion signal intensity of muon capture interfacial migration light induced electron initiation photochemical reaction products therefrom simultaneously pass through image Reconstruct obtains the micro-imaging in photocatalytic activity site, on the one hand may determine that semi-conducting material photocatalytic activity site areas, On the other hand it can also judge that photochemically reactive difficulty or ease occur for electron acceptor molecule (substance) and to analyze and identify gained photochemical Learn reaction product.
(2) compared with existing Fluorescence Spectrometer, the present invention generates light induced electron using semi-conducting material under laser irradiation Macroscopical tunnel-effect and electron acceptor molecule capture principle, measure electron acceptor molecule capture interfacial migration light induced electron or Electron acceptor molecule captures the photochemical reaction product that interfacial migration light induced electron causes, since time-of-flight mass analyzer has There is full scan function, electrostatic field size is adjustable, and delay is adjustable, and optical maser wavelength, spot size, pulse frequency and width are also adjustable, Therefore, it is substantially increased to light induced electron transfer and various light-catalyzed reaction products using four-dimensional microscopic image analysis instrument of the invention Detectability, overcome the detection limitation of fluorescent spectrometry.
(3) with existing scanning electron microanalyzer necessarily require sample in high vacuum state compared with, the present invention can survey Photoelectron transfer and the photochemical reaction for determining interface under atmospheric pressure state, can be under the conditions of real reaction to photocatalytic activity position Point carries out micro-imaging;And assay method of the present invention can carry out the real time measure under atmospheric conditions, can reflect interface light Change with time situation for electronics transfer and photocatalytic activity site, is conducive to commercial application.
(4) operating process of test method of the present invention is easy to control, and analyze speed is fast, and background interference is small, radiationless Or Pollution by Chemicals, spatial resolution is high, and mass accuracy is high, and property is stablized, particularly suitable for semiconductor material interface electronics The measurement and microscopic image analysis of transfer and photocatalytic activity are convenient for quality control and industrialization.
(5) the four-dimensional microscopic image analysis instrument in the present invention for the transfer of interface photoelectron and material light catalysis determination of activity Novel design, composition is simple and easy to get, and used reagent and parts are environmentally protective, and friendly interface is safe and practical.
Description of the drawings
Fig. 1 is the schematic diagram of four-dimensional microscopic image analysis instrument, and 1 is sample target, and 2 be laser, and 3 be slit, and 4 be extraction Pole, 5 be six grades of bars, and 6 be level four bars, and 7 be time-of-flight mass analyzer, and 8 be detector, and 9 be the device for providing voltage.
Fig. 2 is four-dimensional microscopic image analysis instrument operating diagram.
Fig. 3 is the anion spectrogram obtained in different electrostatic fields under anionic textiles pattern of embodiment 1.
Fig. 4 is the negative ion mode under the cation spectrogram and anionic textiles pattern obtained under positive ion detection pattern, Voltage difference is 0.1 volt wherein between sample target and slit, and abscissa is mass-to-charge ratio in spectrogram, and ordinate is signal strength.
Fig. 5 is embodiment 2 under positive ion detection pattern, and voltage difference is 60 volts of electrostatic field between sample target and slit In obtained cation spectrogram.
Fig. 6 is using Nucin as electron acceptor molecule in embodiment 3, in titanium dioxide exposure<100>It is brilliant The photocatalytic activity micro-imaging in face and side.
Fig. 7 is embodiment 4 with persistence organochlorine pollutant 4 in typical environment, and 4 '-DDT are electron acceptor molecule, two Titanium oxide exposure<100>The photocatalytic activity micro-imaging of crystal face and side.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention Content is not limited solely to the following examples.
As depicted in figs. 1 and 2, it is a kind of for measure interface photoelectron transfer and the active four-dimension of material light catalysis it is micro- at As analyzer, including the sample target, laser, slit, extraction pole, six grades of bars, level four bars, the time of flight mass that are sequentially arranged divide Parser and detector, further include the device that voltage is provided to sample target, slit, extraction pole and six grades of bars, and the laser is used for To sample target emission pulse laser, there are electrostatic field, the time-of-flight mass analyzer between the sample target~six grade bar For measuring ion mass-to-charge ratio, the detector is for detecting ion signal intensity and then obtaining photocatalysis by image reconstruction The micro-imaging of active site.The sample target and laser are in sample bin, and sample bin is atmospheric pressure;It is described narrow Seam, extraction pole, six grades of bars, level four bars, time-of-flight mass analyzer and detector are in vacuum system.
Further, can also electrostatic electron lens be set in sample bin, between sample target and slit, is used for ion Focusing and transmission.Further, the four-dimensional microscopic image analysis instrument further includes control system, for controlling pulse laser The synchronous or delay with electrostatic field.
Embodiment 1
The assay method in the photoelectron transfer of titania nanoparticles surface and photocatalytic activity site, including walk as follows Suddenly:
(1) preparation of titanium dioxide semiconductor nano material suspension:It weighs 10mg nano materials and is dissolved in 1mL isopropanols In, ultrasonic vibration 1 minute keeps nano particle evenly dispersed;
(2) electron acceptor molecule solution is prepared:It weighs 100mg Nucins to be dissolved in 1mL acetone, prepare Obtain electron acceptor molecule solution;
(3) cleaning sample target takes 1 microlitre of titanium dioxide semiconductor nano material hanging drop on sample target, dries in the air naturally It is dry;Take 1 microlitre of electron acceptor molecule solution drop in titanium dioxide semiconductor nano-material surface, naturally dry;
(4) sample target is put into four-dimensional microscopic image analysis instrument, under anionic textiles pattern, adjust sample bin humidity and Temperature adjusts sample target, slit, six grades of bars, the voltage on extraction plate, makes the voltage difference between sample target and slit be respectively 20,30,60 volts;
(5) setting laser parameter (optical maser wavelength is set as 355nm), laser photon energy should be greater than the energy of semi-conducting material Gap;Laser is opened to sample target emission pulse laser, synchronous to open electrostatic field, semi-conducting material generates interfacial migration photoproduction electricity Son, electron acceptor molecule capture interfacial migration light induced electron and form anion or electron acceptor molecule capture interfacial migration photoproduction electricity Son causes the fracture of specific chemical key and obtains fragment anion, and gained anion is moved to high potential direction in electrostatic field, worn It crosses slit, extracted plate, six grades of bars and level four bars to focus, mass-to-charge ratio is finally measured by time-of-flight mass analyzer, by detecting Device detects ion signal intensity, and gathered data obtains the micro-imaging in photocatalytic activity site by image reconstruction.
(6) by spectrogram C6 obtained by step (5):0, C8:0, C10:0, C12:0, C14:0, C16:0, C18:0, C20:0 He C22:0 exact mass is corrected.
In the present embodiment, the voltage difference between sample target and slit is respectively the spectrogram of gained under 20,30,60 volts as schemed Shown in 3, as can be seen from Figure 3:When voltage difference is 20V, 30V, 60V, electron acceptor molecule captures the photoproduction electricity of interfacial migration Submode includes mating type electron capture and dissociation type electron capture (generating different fragment ions).
In the present embodiment, the voltage difference between sample target and slit is set as 0.1V, respectively in positive ion mode and negative The mass-to-charge ratio spectrogram of ion is detected under ion mode, the results are shown in Figure 4, and Fig. 4 (A) is the spectrogram under negative ion mode, Fig. 4 (B) it is the spectrogram under positive ion mode, generated anion passes through electrostatic first after electron acceptor molecule capture light induced electron Interaction combines a proton, and then the atom with lone pair electrons is in conjunction with a proton, therefore total electrical charge number is+1, from Fig. 4 (A) and Fig. 4 (B) can be seen that:It is anion that the light induced electron of electron acceptor molecule capture interfacial migration, which is formed by, It just confirms under the voltage difference of 0.1V, the mode that electron acceptor molecule captures the light induced electron of interfacial migration is mating type electronics Capture.
Embodiment 2
Four-dimensional microscopic image analysis instrument is also switched under positive ion detection pattern by the present embodiment, to nano titania The transfer of grain surface photoelectron and photocatalytic activity site are measured, specific method with embodiment 1, the difference is that:Just Under ion detection mode, the voltage difference between sample target and slit is designed as 50V, and the cation spectrogram of gained is as shown in figure 5, figure 5 illustrate that electron detachment has occurred in electron acceptor molecule.
Embodiment 3
The present embodiment determines titanium dioxide exposure<100>Crystal face and side light electronics transfer and photocatalytic activity position Point, specific assay method with embodiment 1, the difference is that, the preparation of sample target:It is soaked with Nucin solution Bubble covering titanium dioxide exposure<100>Crystal face and side will adsorb the viscous titanium dioxide exposure of Nucin <100>Crystal face and side are fixed on conductive metallic aluminium band or copper strips;Voltage difference between sample target and slit is designed as 20V.It is detected as shown in fig. 6, as can be seen from Figure 6:Titanium dioxide exposure<100>The micro imaging signals of crystal face are very It is low, illustrate that photocatalytic activity is poor, and its side is (non-<100>Crystal face) show very strong micro-imaging, illustrate have compared with More photocatalytic activity sites.
Embodiment 4
With persistence organochlorine pollutant 4 in typical environment, 4 '-DDT are electron acceptor molecule, and detection 4,4 '-DDT are two Titanium oxide exposure<100>Micro-imaging on the photocatalytic activity site of crystal face and side, includes the following steps:
(1) electron acceptor molecule solution is prepared:100mg4,4 '-DDT are weighed, are dissolved in 1mL acetone;
(2) 4,4 '-DDT solution obtained by step (1) is used to impregnate covering titanium dioxide crystal surface, naturally dry;
(3) titanium dioxide crystal obtained by step (2) is pasted onto aluminium strip or copper strip surface, be then attached to through over cleaning Sample target on, make<100>Crystal face is upward;
(4) sample target is put into four-dimensional microscopic image analysis instrument, under anionic textiles pattern, adjust sample bin humidity and Temperature sets electrostatic electron lens parameter, adjusts sample target, slit, six grades of bars, the voltage on extraction plate, makes sample target and narrow Voltage difference between seam is respectively 20 volts.
(5) setting laser parameter (optical maser wavelength is set as 355nm), laser photon energy should be greater than the energy of semi-conducting material Gap;Laser is opened to sample target emission pulse laser, synchronous to open electrostatic field, semi-conducting material generates interfacial migration photoproduction electricity Son, electron acceptor molecule capture interfacial migration light induced electron and obtain anion, and gained anion is in electrostatic field to high potential side To movement, slit, extracted plate, six grades of bars and level four bars is passed through to focus, matter lotus is finally measured by time-of-flight mass analyzer Than detecting ion signal intensity, gathered data by detector;
(6) by spectrogram C6 obtained by step (5):0, C8:0, C10:0, C12:0, C14:0, C16:0, C18:0, C20:0 He C22:0 exact mass is corrected, and obtains 4 by image reconstruction, 4 '-DDT are captured obtained by photoelectron and light-catalyzed reaction The micro-imaging of anion.
In the present embodiment, the voltage difference between sample target and slit is respectively the micro-imaging figure of gained under 20 volts as schemed Shown in 7, as can be seen from Figure 7:4,4 '-DDT can capture the light induced electron of interfacial migration, capture side as electron acceptor molecule Formula includes mating type electron capture and dissociation type electron capture, and it is anti-that photochemistry has occurred after 4,4 '-DDT molecules capture light induced electron It answers, the fracture of chemical bond has occurred, produce fragment ion (photochemical reaction product).
Obviously, above-described embodiment be only intended to clearly illustrate made by example, and not limitation to embodiment.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified It moves within still in the protection domain of the invention.

Claims (7)

1. one kind exists for measuring interface photoelectron transfer and the active four-dimensional microscopic image analysis instrument of material light catalysis, feature In, including be sequentially arranged sample target, laser, slit, extraction pole, six grades of bars, level four bars, time-of-flight mass analyzer and Detector, further includes the device that voltage is provided to sample target, slit, extraction pole and six grades of bars, and the laser is used for sample Target emission pulse laser, there are electrostatic fields between the sample target ~ six grade bar, and the time-of-flight mass analyzer is for measuring Ion mass-to-charge ratio, the detector is for detecting ion signal intensity and then obtaining photocatalytic activity site by image reconstruction Micro-imaging;The sample target and laser are in sample bin, and sample bin is atmospheric pressure;The slit, extraction pole, Six grades of bars, level four bars, time-of-flight mass analyzer and detector are in vacuum system;The four-dimension microscopic image analysis instrument When being under anionic textiles pattern, anion moves in electrostatic field to high potential direction, passes through slit, extracted pole, six Grade bar and level four bars focus, and finally measure ion mass-to-charge ratio by time-of-flight mass analyzer, ion signal is detected by detector Intensity and the micro-imaging that photocatalytic activity site is obtained by image reconstruction;Under positive ion detection pattern, cation Moved to low potential direction in electrostatic field, slit, extracted pole, six grades of bars and level four bars passed through to focus, finally by flight when Between mass analyzer measure ion mass-to-charge ratio, detected by detector and ion signal intensity and photocatalysis obtained by image reconstruction The micro-imaging of active site.
2. according to claim 1 for measuring interface photoelectron transfer and the active four-dimensional micro-imaging of material light catalysis Analyzer, which is characterized in that electrostatic electron lens is set between sample target and slit, is used for the focusing and transmission of ion, institute It states electrostatic electron lens to be in sample bin, sample bin is atmospheric pressure.
3. according to claim 1 for measuring interface photoelectron transfer and the active four-dimensional micro-imaging of material light catalysis Analyzer, which is characterized in that the four-dimension microscopic image analysis instrument further includes control system, for controlling pulse laser and electrostatic The synchronization or delay of field.
4. measuring the transfer of interface photoelectron using any four-dimensional microscopic image analysis instrument of claim 1 ~ 3 and material light being urged Change active method, which is characterized in that include the following steps:
(1)Set laser parameter:According to the property of semi-conducting material and energy gap size, correspondingly optical maser wavelength is selected, material is made Energy gap is less than laser photon energy;
(2)Set electrostatic field parameters:Electrostatic field, sample target and narrow are set according to the property of semi-conducting material and electron acceptor molecule The light induced electron that voltage difference between seam can be such that semiconductor material surface generates obtains enough energy and occurs tunnelling, and electronics by The ion generated after body molecule capture photoelectron is focused in the electrostatic field between-six grades of bars of slit and transmission;The semiconductor Material is selected from SiO2、BiOCl、Ce2O3、BN、AlN、TiO2And Ga2O3In one kind;The electron acceptor molecule is selected from 5- hydroxyls- 1,4- naphthoquinones or 4,4 '-DDT;
(3)Prepare semi-conducting material suspension to be measured;Or the semi-conducting material of different crystal faces is pasted on to conductive metallic aluminium band Or the semi-conducting material exposed with a variety of crystal faces is prepared on copper strips;
(4)Cleaning sample target draws semi-conducting material hanging drop to be measured in sample target surface, then naturally dry is partly being led Electron acceptor molecule solution, naturally dry is added dropwise in body material surface;Or covering is impregnated with more with electron acceptor molecule solution The semi-conducting material of kind crystal face exposure will adsorb half with the exposure of a variety of crystal faces of electron acceptor molecule after natural drying Conductor material is fixed on sample target, and crystal face to be measured is upward;
(5)Sample target is put into sample bin, laser is opened to sample target emission pulse laser, adjusts electrostatic field, make semiconductor Material generates interfacial migration light induced electron, and electron acceptor molecule obtains cation after capturing interfacial migration light induced electron and/or bears Ion;
(6)Under anionic textiles pattern, step(5)Middle gained anion moves in electrostatic field to high potential direction, It is focused across slit, extracted pole, six grades of bars and level four bars, ion mass-to-charge ratio is finally measured by time-of-flight mass analyzer, Ion signal intensity is detected by detector and obtains the micro-imaging in photocatalytic activity site by image reconstruction;When in just Under ion detection mode, step(5)Middle gained cation moves in electrostatic field to low potential direction, passes through slit, extracted Pole, six grades of bars and level four bars focus, and finally measure ion mass-to-charge ratio by time-of-flight mass analyzer, ion is detected by detector Signal strength and the micro-imaging that photocatalytic activity site is obtained by image reconstruction.
5. measurement interface according to claim 4 photoelectron shifts and the active method of material light catalysis, which is characterized in that The electron acceptor molecule capture interfacial migration light induced electron includes that mating type electron capture, dissociation type electron capture and electronics are de- From.
6. measurement interface according to claim 5 photoelectron shifts and the active method of material light catalysis, which is characterized in that The mating type electron capture is to form anion after electron acceptor molecule captures light induced electron;The dissociation type electron capture is Electron acceptor molecule causes specific chemical key fracture acquisition fragment anion after capturing light induced electron, and the electron detachment is height Electron detachment occurs and obtains cation after the light induced electron of speed movement and electron acceptor molecule interaction.
7. measurement interface according to claim 4 photoelectron shifts and the active method of material light catalysis, which is characterized in that Wavelength, spot size, pulse frequency, pulse width, the laser incident angle of the laser are tunable, and pulse laser can be with Electrostatic field synchronization or delay.
CN201610887230.3A 2016-09-28 2016-10-11 A kind of transfer of interface photoelectron and the active assay method of material light catalysis and four-dimensional microscopic image analysis instrument Active CN106323921B (en)

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